US2988853A - Glass-to-metal seal - Google Patents

Glass-to-metal seal Download PDF

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Publication number
US2988853A
US2988853A US678565A US67856557A US2988853A US 2988853 A US2988853 A US 2988853A US 678565 A US678565 A US 678565A US 67856557 A US67856557 A US 67856557A US 2988853 A US2988853 A US 2988853A
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US
United States
Prior art keywords
nickel
oxide
ferrule
glass
eyelet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US678565A
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English (en)
Inventor
Anthony J Certa
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Maxar Space LLC
Original Assignee
Philco Ford Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to DENDAT1252035D priority Critical patent/DE1252035B/de
Priority to BE570133D priority patent/BE570133A/xx
Application filed by Philco Ford Corp filed Critical Philco Ford Corp
Priority to US678565A priority patent/US2988853A/en
Priority to FR1207744D priority patent/FR1207744A/fr
Priority to GB26287/58A priority patent/GB895778A/en
Application granted granted Critical
Publication of US2988853A publication Critical patent/US2988853A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • H10W76/161—
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/04—Joining glass to metal by means of an interlayer
    • C03C27/042—Joining glass to metal by means of an interlayer consisting of a combination of materials selected from glass, glass-ceramic or ceramic material with metals, metal oxides or metal salts
    • C03C27/046—Joining glass to metal by means of an interlayer consisting of a combination of materials selected from glass, glass-ceramic or ceramic material with metals, metal oxides or metal salts of metals, metal oxides or metal salts only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
    • C23D3/00—Chemical treatment of the metal surfaces prior to coating
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J5/00—Details relating to vessels or to leading-in conductors common to two or more basic types of discharge tubes or lamps
    • H01J5/20—Seals between parts of vessels
    • H01J5/22—Vacuum-tight joints between parts of vessel
    • H01J5/26—Vacuum-tight joints between parts of vessel between insulating and conductive parts of vessel
    • H10W72/00—
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2893/00—Discharge tubes and lamps
    • H01J2893/0033—Vacuum connection techniques applicable to discharge tubes and lamps
    • H01J2893/0037—Solid sealing members other than lamp bases
    • H01J2893/0041—Direct connection between insulating and metal elements, in particular via glass material
    • H01J2893/0043—Glass-to-metal or quartz-to-metal, e.g. by soldering

Definitions

  • this invention is especially useful in the making of semiconductor devices, such as transistors.
  • the eld relating to the production of glass-to-metal seals is highly developed and one of rapidly increasing import, having extensive application in electronics and related industries. Notwithstanding the intense activity in this ield and a present latitude in ⁇ choice of suitable glasses and metals to produce the type of seal desired, there has been no adequate technique for producing an effective glass-to-nickel seal.
  • Nickel because of its highly porous structure readily occludes air and characteristically produces a gassy seal. This problem, which manifests itself in some degree in numerous metals, can usually be alleviated by preheating the rnetal in a vacuum or in a protective atmosphere. Paradoxically, however, in the case of nickel, heating at elevated temperatures serves to disrupt the sheath of oxide formed on the surface of the body of nickel, which iilm is indispensable to the proper bonding of the glass to the nickel.
  • Another and equally important object olf this invention is to provide a method of oxidizing nickel which will produce a strongly adherent film of oxide on the surface of the nickel and one which is relatively undisturbed by temperatures normally employed in the glassing process, in addition to being readily wetted by refractory glasses and other vitreous materials.
  • a subordinate obje'ct of this invention ⁇ is to provide a simple, inexpensive method for obtaining the desired film of oxide on the surface of a body of nickel.
  • oxide as used herein is to be broadly construed and is to be understood asencompassing such compounds and intermixtures .of nickel as result from the practice of the method steps 2,988,853 Patented June 20, 1961 of this invention, and does not necessarily refer to a specic lcompound.
  • FIGURE l depicts an encapsulated transistor embodying seals made in accordance with the technique of the present invention
  • FIGURE 2 is an enlarged fragmentary showing of a transistor stem eyelet, of the type shown in FIG. 1, before undergoing treatment in accordance with the meth- 0d steps of this invention;
  • FIGURE 3 is a somewhat ⁇ diagrammatic illustration of one form of apparatus adapted for use in carrying out the method steps of this invention
  • FIGURE 4 shows the transistor s-tem eyelet depicted in FIGURE 2 after having been treated, in accordance with the method steps of this invention, and;
  • FIGURE 5 is an enlarged fragmentary showing of the completed transistor stern assembly depicting the hermetic sealing of the stem eyelet and lead wires.
  • the method of this invention comprises heating the body of nickel in an oxidizing atmosphere to a temperature lying in the range from about l000 C., as a lower limit, to a value just under the melting point of nickel, as a higher limit, maintaining the body of nickel at this elevated temperature for la predetermined length of time, dependent for example upon the thickness of oxide desired, and then cooling said body in such manner as to prevent further oxidation, this being desirably accomplished by rapid cooling, as by Iliquid quenching.
  • further oxidation of the ynickel is prevented by simply allowing the heated body of nickel to cool slowly in an inert atmosphere such as gaseous nitrogen.
  • FIGURE l of the drawing illustrating an enlarged sectional view of a conventional transistor 10, the unit including the housing or can 11, hermeti'cally sealed by the stem assembly 12.
  • This latter assembly consists of the eyelet 13, insulating core 14 and lead-in wires 15, all of the elements being hermetically bonded to the vitric core 14.
  • the can in order to resist corrosion is made of nickel, and while it is highly advantageous to also make the eyelet 13 of nickel, in order to facilitate the bold welding of these members, it has heretofore been impractical because of prior art limitations in forming an effective bond between the nickel eyelet 13 and the insulating vitric core 14.
  • Soldering techniques while not producing contaminants of the nature mentioned above, fail to provide an hermetic seal which will remain reliable under the extreme environmental conditions to which these units are customarily subjected. Means permitting the highly desirable use of nickel to facilitate the desired cold welding of the transistor encapsulating members have consequently been the subject of considerable investigation.
  • the method teachings of this invention solve the presently existing impasse by enabling vitrie materials, such as glass, Vto be hermetically sealed to nickel through the intermediary of a readily wetted, tenaciously adherent, lrn of oxide formed on the surface of the parent metal.
  • the stem eyelet 13, shown in FIG. 2, is made of nickel, or a high nickel alloy, which, for most effective treatment, is iirst surface-cleaned by using trichlorethylene or other suitable reagents.
  • This step is desirably followed by a bright dip which removes any latent oxide iilrn from the parts.
  • a typical bright dip composition may be made by using 1125 ml. of HNO3, 750 ml. of H2804 and 500 ml. of H2O, to which 6 grams of NaCl are added per liter of solution.
  • the parts may be iired in a hydrogen atmosphere at approximately 900 degrees to insure the removal of undesirable oxides. Any of numerous commercially recognized techniques, of which the above are exemplary, may be employed to obtain a body of nickel substantially free of surface contaminants.
  • This step while not indispensable to the method teachings of the invention, is highly desirable if consistently satisfactory results are to be obtained.
  • the eyelet 13, after cleaning is then heated in any suitable manner as by being placed in the oven 17 shown in FIG. 3.
  • a plurality of eyelets are positioned on a suitable support 18 located within the oven enclosure 19.
  • the oven is then heated to prescribed temperature by energization of the resistive element 20.
  • Experimentation has established the fact that it is necessary to fire the parts undergoing oxidation to a temperature at least in the region of 1000 C. in order to obtain a consisently adherent, wettable oxide film, and preferably above 1050 C. Desirably the parts are maintained at this elevated temperature for several minutes, the time, however, is not critical and is best determined by experimentation.
  • lt was found, for example, that excellent seals could be made to a nickel eyelet formed of 15 mil stock having an over-all length of 100 mils and an inside diameter of 150 mils by heating the eyelet for six minutes at a temperature of l050 C., or for three minutes at a temperature of 1075 C. Equally eifective results were obtained however by varying the temperature and xing the time at some nominal ligure such as 10 minutes. It should be nonetheless recognized that the temperature must be no CTI lower than the minimum level specified above and that by this latter method being equally as satisfactory as that resulting from rapid cooling.
  • the rapid' temperature reduction referred to above may be accomplished using any number of materials, the wide choice of suitable materials making it clearY that the ultimately resulting oxide formation is not brought about as a result of chemical reaction between the nickel and some constituent found in the quenching media. Equally satisfactory results were obtained, for example, using water, glycerol, acetone, mineral oil, or borating solution, these materials being merely illustrative of the types of quenches available and in no way restrictive thereof.
  • a body of nickel oxidized in accordance with the method steps of this invention exhibits a sheath of oxide having a color from gray-green to green.
  • nickel oxidizes to either monoxide or dioxide, each of these materials being susceptible to analysis by chemical means.
  • the oxide formed by the disclosed process does not yield to either the monoxide or dioxide tests, the resulting material being possibly an intimate admixture of both forms of oxide.
  • the nickel lead-in wires 15 are oxidized in a manner similar to that employed in the oxidation of the eyelets 13. These parts are then hermetically sealed within the core matrix as shown most clearly in FIGURE 5, the fabrication being desirably accomplished in accordance with the method disclosed ⁇ and claimed in the copending application of Henry P. Beerman and Ford K. Clarke, bearing Serial No. 654,907 tiled April 24, 1957, and assigned to the assignee of the present invention.
  • This method consists of compacting fusible insulating material, such as Dow Corning G-12, in granulated form, whose composition was known prior to the present invention and having an oxide composition approximating that set out below, around the leads 15 disposed in :oriented relation within the eyelet 13, the technique resulting in a mechanical integration of the particles and serving to produce suiciently intimate contact between the leads and core material to effect, on subsequent heating to a temperature in the region of approximately 900 C., hermetic juncture of the constituent parts.
  • the resulting seal has a bubble-free interface of generally greenish appearance.
  • the invention from a method aspect comprises oxidizing a body of nickel by heating to a temperature of approximately 1000 C. and then retaining the desired oxide thus formed by cooling in such a manner as to prevent further change in the oxide formation.
  • This latter step can be accomplished by either cooling the nickel rapidly enough to inhibit the formation of further oxide or by allowing the nickel to cool in an inert atmosphere thereby preventing further oxidation.
  • stems for hermetically sealed semiconductor devices of the type including a nickel ferrule housing an insulating core of vitric material
  • the method whichcomprises: elevating the temperature of said ferrule in an oxidizing atmosphere to a value lying in the range above approximately 1000 C. but below the melting point of nickel; maintaining said ferrule in said elevated temperature range for a period of time sufficient to produce a layer of oxide of predetermined thickness; liquid quenching said ferrule to cool it in a manner preventing further oxidation; and thereafter completing the stem assembly by hermetically joining said vitric core to said cooled ferrule.
  • the method of fabricating glass-to-nickel seals which comprises: heating a body of nickel in an oxidizing atmosphere to a temperature lying in the range above approximately 1000 C. but below the melting point of nickel; maintaining said body Within said elevated temperature range for a period of time suiiicient to produce an oxide layer of predetermined thickness; quenching said body to cool it in a non-oxidizing environment; and thereafter forming a glass to nickel seal.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Joining Of Glass To Other Materials (AREA)
  • Glanulating (AREA)
US678565A 1957-08-16 1957-08-16 Glass-to-metal seal Expired - Lifetime US2988853A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
DENDAT1252035D DE1252035B (index.php) 1957-08-16
BE570133D BE570133A (index.php) 1957-08-16
US678565A US2988853A (en) 1957-08-16 1957-08-16 Glass-to-metal seal
FR1207744D FR1207744A (fr) 1957-08-16 1958-07-09 Joint nickel-verre
GB26287/58A GB895778A (en) 1957-08-16 1958-08-15 Improvements in and relating to the oxidation of nickel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US678565A US2988853A (en) 1957-08-16 1957-08-16 Glass-to-metal seal

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US2988853A true US2988853A (en) 1961-06-20

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US678565A Expired - Lifetime US2988853A (en) 1957-08-16 1957-08-16 Glass-to-metal seal

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US (1) US2988853A (index.php)
BE (1) BE570133A (index.php)
DE (1) DE1252035B (index.php)
FR (1) FR1207744A (index.php)
GB (1) GB895778A (index.php)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3107530A (en) * 1959-04-06 1963-10-22 Borg Warner Temperature sensing apparatus
US3281309A (en) * 1961-12-12 1966-10-25 Gen Electric Ceramic bonding
US3370991A (en) * 1963-05-31 1968-02-27 Corning Glass Works Method of preoxidation of stainless steel
US3445210A (en) * 1964-03-05 1969-05-20 Fujitsu Ltd Adhesive material and method of using same to adhere ceramic material to metal
US3635510A (en) * 1969-11-20 1972-01-18 Rca Corp Heat seal of a glass member to another member
US4012239A (en) * 1972-11-21 1977-03-15 Union Siserurgique du Nord et de l'Est de la France, par abreviation "USINOR" Process for treating steel sheets for the purpose of enamelling the sheets
US5522003A (en) * 1993-03-02 1996-05-28 Ward; Robert M. Glass preform with deep radial gradient layer and method of manufacturing same

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3345218A (en) * 1964-04-02 1967-10-03 Owens Illinois Inc Preoxidation of stainless steel for glass-to-metal sealing
US4405670A (en) * 1982-05-28 1983-09-20 Rca Corporation Capacitance electronic disc stamper having improved stain resistance and method for the manufacture thereof

Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1823179A (en) * 1929-09-09 1931-09-15 Aluminum Co Of America Aluminum type matrix
US1901563A (en) * 1926-09-16 1933-03-14 Westinghouse Electric & Mfg Co Copper oxide rectifier
US1955564A (en) * 1931-10-14 1934-04-17 Gen Electric Electric current rectifier
US2010145A (en) * 1932-12-09 1935-08-06 Heints & Kaufman Ltd Metal-to-glass seal
US2103610A (en) * 1935-04-30 1937-12-28 Sofal Ltd Alloy steels
US2148664A (en) * 1935-07-15 1939-02-28 Degussa Heat treatment of metals
US2193640A (en) * 1938-05-21 1940-03-12 Gen Electric Glass-to-metal seal
US2206392A (en) * 1938-06-14 1940-07-02 Int Nickel Co Process of producing colored oxide coatings on nickel and nickel alloys
US2266117A (en) * 1938-07-16 1941-12-16 Int Nickel Co Process of producing colored oxide coatings on nickel and nickel alloys
US2371627A (en) * 1939-04-25 1945-03-20 Sylvania Electric Prod Composite glass-metal alloy article
US2422628A (en) * 1943-06-12 1947-06-17 Sylvania Electric Prod Glass to metal seal
GB589881A (en) * 1944-10-18 1947-07-02 Sylvania Electric Prod Improvements in oxidation of stainless steel
US2446277A (en) * 1945-09-24 1948-08-03 Eitel Mccullough Inc Glass to metal seal in electrical devices
US2461935A (en) * 1943-08-14 1949-02-15 Int Nickel Co Insulated electrical resistances
US2513302A (en) * 1945-02-17 1950-07-04 Armco Steel Corp Black oxide coated nitrided stainless steel product
US2584354A (en) * 1951-01-11 1952-02-05 Rca Corp Method of sealing a glass facing to a surface of a metal body
US2709145A (en) * 1950-11-23 1955-05-24 Int Nickel Co Heat-treatment of nickel and nickel containing alloys
US2743553A (en) * 1951-11-26 1956-05-01 Corning Glass Works Metal sealing glass and seal

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1901563A (en) * 1926-09-16 1933-03-14 Westinghouse Electric & Mfg Co Copper oxide rectifier
US1823179A (en) * 1929-09-09 1931-09-15 Aluminum Co Of America Aluminum type matrix
US1955564A (en) * 1931-10-14 1934-04-17 Gen Electric Electric current rectifier
US2010145A (en) * 1932-12-09 1935-08-06 Heints & Kaufman Ltd Metal-to-glass seal
US2103610A (en) * 1935-04-30 1937-12-28 Sofal Ltd Alloy steels
US2148664A (en) * 1935-07-15 1939-02-28 Degussa Heat treatment of metals
US2193640A (en) * 1938-05-21 1940-03-12 Gen Electric Glass-to-metal seal
US2206392A (en) * 1938-06-14 1940-07-02 Int Nickel Co Process of producing colored oxide coatings on nickel and nickel alloys
US2266117A (en) * 1938-07-16 1941-12-16 Int Nickel Co Process of producing colored oxide coatings on nickel and nickel alloys
US2371627A (en) * 1939-04-25 1945-03-20 Sylvania Electric Prod Composite glass-metal alloy article
US2422628A (en) * 1943-06-12 1947-06-17 Sylvania Electric Prod Glass to metal seal
US2461935A (en) * 1943-08-14 1949-02-15 Int Nickel Co Insulated electrical resistances
GB589881A (en) * 1944-10-18 1947-07-02 Sylvania Electric Prod Improvements in oxidation of stainless steel
US2513302A (en) * 1945-02-17 1950-07-04 Armco Steel Corp Black oxide coated nitrided stainless steel product
US2446277A (en) * 1945-09-24 1948-08-03 Eitel Mccullough Inc Glass to metal seal in electrical devices
US2709145A (en) * 1950-11-23 1955-05-24 Int Nickel Co Heat-treatment of nickel and nickel containing alloys
US2584354A (en) * 1951-01-11 1952-02-05 Rca Corp Method of sealing a glass facing to a surface of a metal body
US2743553A (en) * 1951-11-26 1956-05-01 Corning Glass Works Metal sealing glass and seal

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3107530A (en) * 1959-04-06 1963-10-22 Borg Warner Temperature sensing apparatus
US3281309A (en) * 1961-12-12 1966-10-25 Gen Electric Ceramic bonding
US3370991A (en) * 1963-05-31 1968-02-27 Corning Glass Works Method of preoxidation of stainless steel
US3445210A (en) * 1964-03-05 1969-05-20 Fujitsu Ltd Adhesive material and method of using same to adhere ceramic material to metal
US3635510A (en) * 1969-11-20 1972-01-18 Rca Corp Heat seal of a glass member to another member
US4012239A (en) * 1972-11-21 1977-03-15 Union Siserurgique du Nord et de l'Est de la France, par abreviation "USINOR" Process for treating steel sheets for the purpose of enamelling the sheets
US5522003A (en) * 1993-03-02 1996-05-28 Ward; Robert M. Glass preform with deep radial gradient layer and method of manufacturing same
US5673353A (en) * 1993-03-02 1997-09-30 Ward; Robert M. Fiber and lens preform with deep radial gradient layer and method of manufacturing same

Also Published As

Publication number Publication date
BE570133A (index.php)
GB895778A (en) 1962-05-09
FR1207744A (fr) 1960-02-18
DE1252035B (index.php) 1967-10-12

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